HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → HCID 66858297, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 66859694 | HCID 66859694 | — |
| Catalyst | Dichloronickel;hexahydrate | HCID 11791229 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66858297 | HCID 66858297 | 69.3% |
Reaction Steps
To a solution of the compound 74 (350 mg) in tetrahydrofuran (4.0 mL) and n-butanol (1.30 mL) was nickel chloride hexahydrate (246 mg) at room temperature and then thereto was added sodium borohydride (156 mg) at 0° C. The solution was stirred for 1 hour. The reaction solution was diluted with ethyl acetate and filtrated through Celite (Brand name). The obtained filtrate was washed an aqueous saturated ammonium chloride solution and brine, dried over anhydrous sodium sulfate and concentrated. The obtained residue was purified by column chromatography on silica gel (ethyl acetate:methanol=1:019:1) to give the title compound (244 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501793B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-9c03cd59ac59423fbc64dc428831ee65 |
| Source note | uspto-grants-2013_08 |